HRID1889087

反应详情

EQUATION

反应方程式

HRID 1889087 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 4-{[2-chloro-3-(trifluoromethyl)phenyl]carbonyl}-2-piperazinone (I1) (0.307 g, 1 mmol) in dry Dichloromethane (DCM) (3 ml) was added triethyloxonium tetrafluoroborate (0.209 g, 1.100 mmol). The solution was then stirred at room temperature and under argon for 30 minutes. 1,2,4-Thiadiazole-5-carbohydrazide (I80) (0.144 g, 1.000 mmol) was then added and the solution was stirred for 1 hour, before the solvent was concentrated and n-BuOH (3.00 ml) was added. The solution was then stirred under argon and reflux for a further 3 hours. The solution was then allowed to cool to room temperature before the solvent was evaporated in vacuo.

WORKUP

后处理

  1. stirringthe solution was stirred for 1 hour, before the solvent
  2. concentrationwas concentrated
  3. additionn-BuOH (3.00 ml) was added
  4. stirringThe solution was then stirred under argon
  5. temperaturereflux for a further 3 hours
  6. temperatureto cool to room temperature before the solvent
  7. customwas evaporated in vacuo